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  • Column liquid chromatography  (349)
  • Coleoptera  (170)
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  • ddc:330
  • Springer  (523)
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  • 1
    ISSN: 1570-7458
    Keywords: Ceutorhynchus constrictus ; Coleoptera ; Curculionidae ; Ceutorhynchinae ; Alliaria petiolata ; garlic mustard ; Brassicaceae ; Cruciferae ; glucosinolates ; sinigrin ; host plant selection ; monophagous ; feeding stimulants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Zusammenfassung Ceutorhynchus constrictus Marsh. (Coleoptera: Chrysomelidae: Ceutorhynchinae) ist ein monophager Rüsselkäfer, der an Knoblauchhederich frisst. Das Wirtswahl-Verhalten dieses Käfers ist im Labor untersucht worden. Die meisten Crucifiren waren im Wahlversuche nicht akzeptiert, wenn Knoblauchhederich als Vergleichspflanze vorhanden war. Von Brassica nigra, Sinapis alba, und Thlaspi arvense wurden im Vergleich gleiche Mengen verzehrt wie von der Wirtspflanze. Blühende Descurainia sophia Pflanzen wurden, im Gegensatz zu Jungpflanzen der gleichen Art, angenommen. Die wichtichsten Phagostimulanten in Extrakten von Knoblauchhederich-Blättern waren ungeladene, wasserlösliche Substanzen. Das häufigste Glukosinolat im Knoblauchhederich, Sinigrin, war auch ein Phagostimulant. Doch war die phagostimulierende Wirkung von Sinigrin nur in Kombinationen mit noch nicht identifizierten, ungeladenen Substanzen aus Knoblauchhederich-Blätter nachweisbar. Wirtspfanzen-Beziehungen von monophagen Insekten werden diskutiert im Zusammenhang mit der Eigenart des Glukosinolat-Inhaltes ihrer Wirtspflanzen.
    Notes: Abstract Host plant relations of the monophagous weevil Ceutorhynchus constrictus Marsh. (Coleoptera: Curculionidae: Ceutorhynchinae) feeding on garlic mustard, Alliaria petiolata (Bieb.) Cavara & Grande (Cruciferae) were studied in the laboratory. Most other crucifers were rejected in choice tests using garlic mustard as a reference plant, but Brassica nigra, Sinapis alba and Thlaspi arvense were as acceptable as the host plant. Flowering plants of Descurainia sophia were acceptable while young plants of this species were not. The most important feeding stimulants in extracts of garlic mustard were uncharged, water soluble compounds. The most abundant glucosinolate in garlic mustard, sinigrin, was a feeding stimulant, too. However, the feeding stimulatory activity of sinigrin was only expressed in the presence of still unidentified uncharged compounds from garlic mustard leaves. Host plant relations in monophagous crucifer-feeding insects is discussed in relation to the distinctness of glucosinolate patterns found in their host plants.
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  • 2
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    Journal of insect behavior 2 (1989), S. 139-141 
    ISSN: 1572-8889
    Keywords: Coleoptera ; Heteroceridae ; egg guarding ; parental care ; predation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
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  • 3
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    Journal of insect behavior 2 (1989), S. 841-847 
    ISSN: 1572-8889
    Keywords: cost of mating ; semelparous ; Photinus collustrans ; Coleoptera ; Lampyridae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
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  • 4
    ISSN: 1570-7458
    Keywords: Aggregation pheromone ; sitophilate ; 1-ethylpropyl 2-methyl-3-hydroxypentanoate ; stereoisomers ; enantiomers ; Sitophilus granarius ; granary weevil ; Coleoptera ; Curculionidae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé S. granarius L. est un déprédateur important des grains stockés. Le (R*,S*)-1-éthylpropyl 2-méthyl-3-hydroxypentanoate a été identifié en 1987 comme le principal composé du sitophilate, la phéromone mâle d'agrégation de S. granarius. La composition énantiométrique du sitophilate a été déterminée par 3 méthodes: 1) tests biologiques des énantiomères synthétiques (2S,3R) et (2R,3S) du diastéréomère actif (R*,S*); 2) spectrométrie RMN 1H des esters Mosher dérivés de la phéromone naturelle et des sitophilates de synthèse (2S*,3R*)-et (2R*,3S*); 3) comparaison en capillarité GLC des temps de rétention des dérivés naturels de la phéromone et des 2 éniantiomères de synthèse. La combinaison des 3 méthodes confirme que le (2S,3R) énantiomère est la forme active du sitophilate. Le mâle produit 〉96% de l'énantiomère (2S,3R). Il n'y a pas eu attraction de S. granarius par le (2R,3S) sitophilate. S. oryzae L. et S. zeamais Motsch n'ont pas été attirés par le (2S,3R)-sitophilate. L'utilisation du (2S,3R)-1-éthylpropyl 2-méthyl-3-hydroxypentanoate dans les pièges devrait permettre une détection précoce de la présence de S. granarius dans des stocks de grains.
    Notes: Abstract The enantiomeric composition of sitophilate, the granary weevil [Sitophilus granarius (L.)] male-produced aggregation pheromone [(R*,S*)-1-ethylpropyl 2-methyl-3-hydroxypentanoate)], was determined by three methods: (1) bioassaying the synthetic (2S,3R) and (2R,3S) enantiomers of the active (R*,S*) diastereomer; (2) 1H NMR spectroscopy of Mosher ester derivatives of the natural pheromone and synthetic (2S,3R)-and (2R,3S)-sitophilate; and (3) capillary GLC comparisons of the retention times of derivatized natural pheromone and the two synthetic enantiomers. The combined methods confirmed the (2S,3R) enantiomer as the active form of sitophilate. Male granary weevils were shown to produce 〉96% (2S,3R)-sitophilate. No significant attraction of S. granarius by the (2R,3S) enantiomer was observed. Rice and maize weevils [S. oryzae (L.) and S. zeamais Motschulsky] were not attracted by (2S,3R)-sitophilate.
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  • 5
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    Entomologia experimentalis et applicata 51 (1989), S. 133-140 
    ISSN: 1570-7458
    Keywords: Coleoptera ; Chrysomelidae ; Leptinotarsa decemlineata ; Colorado potato beetle ; Solanaceae ; Solanum berthaultii ; potato ; plant resistance ; glandular trichomes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé Les mécanismes de défense de la pomme de terre sauvage, S. berthaultii Hawkes, aux larves de Leptinotarsa decemlineata Say, ont été étudiés par ablation sélective des trichomes glandulaires et par l'élimination de leur exsudat des folioles, et par comparaison avec S. tuberosum L. qui a perdu les trichomes glandulaires défensifs A et B. L'ablation des trichomes A a augmenté la proportion de larves ayant consommé S. berthaultii. L'élimination de l'exsudat des trichomes B a augmenté la proportion de consommatrices et réduit la mortalité. Les principaux composés actifs de l'exsudat B, c'est-à-dire des esters d'acides gras de sucrose, n'étaient actifs qu'en présence de trichomes A. Les esters de sucrose n'ont pas modifié la consommation larvaire sur folioles de S. tuberosum, ou sur disques de feuilles de S. berthaultii dont les trichomes A avaient été enlevés. La croissance des larves survivantes n'a pas été modifiée significativement par l'ablation des trichomes A ou l'élimination de l'exsudat de B. La croissance des larves a été significativement augmentée quand les folioles de S. berthaultii ont été incorporés dans l'aliment artificiel après élimination de la barrière physique due aux pédoncules B. La croissance a été de même importance sur aliments artificiels contenant des feuilles (fraiches ou en poudre lyophylisée) de S. berthaultii ou de S. tuberosum, mais plus faible que sur folioles de S. tuberosum. La présence de trichomes A est indispensable à la résistance de S. berthaultii aux L, de L. decemlineata. Les gouttelettes de type B contenant des esters de sucrose augmentent l'expression de la résistance en présence d'une défense active par trichomes A.
    Notes: Abstract The defensive mechanisms of the wild potato, solanum berthaultii Hawkes, to larvae of the Colorado potato beetle, Leptinotarsa decemlineata (Say), were studied by selective removal of glandular trichomes and trichome exudates from leaflets, and by comparing performance on S. berthaultii and on the cultivated potato, S. tuberosum L., which lacks defensively active type A and B glandular trichomes. Removal of type A trichomes increased the proportion of larvae that fed on S. berthaultii. Removal of the exudate from type B trichomes increased the proportion of larvae that fed and led to a decrease in mortality. The predominant active compounds in type B exudate, i.e. fatty acid esters of sucrose, were only effective in the presence of type A trichomes. Sucrose esters did not affect larval feeding on S. tuberosum leaflets or on S. berthaultii leaf discs from which the type A trichomes had been removed. Growth of surviving larvae was not significantly affected by removing type A trichomes or type B exudate. Growth of larvae was significantly increased when S. berthaultii leaflets were presented in artificial diet which eliminated the physical barrier of the type B stalks. Growth was no different on artificial diet containing either S. berthaultii or S. tuberosum leaf material (fresh or lyophilized powder) but was poorer on these diets than on S. tuberosum leaflets. The presence of type A trichomes is a fundamental requirement for expression of S. berthaultii resistance to L1 L. decemlineata. Type B droplets containing sucrose esters increase the expression of resistance in the presence of defensively-active type A trichomes.
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  • 6
    ISSN: 1570-7458
    Keywords: Coleoptera ; Cerambycidae ; Morimus funereus ; development ; laboratory conditions ; food quality ; temperature ; season
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé L'étude a porté sur les effets d'une température constante (23 °C), de la qualité de l'aliment,-B = aliment naturel, c'est-à-dire de l'écorce de chêne pulvérisée; B+C = aliment naturel enrichi avec de la poudre de biscuits sucrés-, et de la saison sur le développement larvaire de M. funereus L. La température de 23 °C a été défavorable aux larves récoltées en septembre dans des souches de chênes et élevées sur aliment B: les larves étaient mortes en 30 jours. Avec aliment B+C, l'effet défavorable a été neutralisé et le poids des larves augmenté de 543%, 897% et 1179% en 1, 2 et 3 mois. Des larves néonates d'été ou d'hiver se sont bien développées sur B+C, mais toutes les larves d'hiver étaient mortes sur B en 40 j. Des larves de mêmes parents, écloses à différentes époques de l'année, ont présenté des différences saisonnières du taux de survie et de la vitesse de développement lors de leur élevage à 23 °C sur B+C. Le développement le plus rapide et la meilleure survie ont été obtenus avec des larves écloses au début ou au milieu de l'été; tandis que le développement le plus lent et la plus mauvaise survie ont été obtenus avec les larves écloses à la fin de l'été. Les changements saisonniers synchrones des adultes et de leurs descendants, exprimés à différents niveaux d'organisation biologique, suggèrent l'existence d'un rythme annuel endogène qui dépend de l'expression de différents gènes au cours du cycle annuel.
    Notes: Abstract The effects of constant temperature (23 °C), food quality (B, natural diet i.e. powdered oak bark; B+C, natural diet enriched with powdered sweet crackers) and season on larval development of the cerambycid Morimus funereus L. were studied. The temperature of 23 °C exerted an unfavourable effect on larvae collected from oak stumps in September and bred on B; i.e. the larvae died within 30 days. When the larvae consumed B+C the unfavourable effect of temperature was abolished and the larvae increased their weight by 543%, 897% and 1179% in 1, 2 and 3 months, respectively. Newly hatched summerand winter-larvae developed successfully on B+C, while all the winter-larvae died within 40 days on B. Larvae of an identical parentage hatched in different phases of the annual cycle and showed seasonal differences in the rate of development and survival when reared on B+C at 23 °C. The fastest development and the highest survival rate were observed in larvae which emerged in early- and midsummer, whereas the slowest development and the lowest survival rate were in those hatched in late summer. The synchronized seasonal changes of adults and their offspring, as expressed at different levels of biological organization, suggest the existence of an endogenous annual rhythm which is dependent upon the expression of different genes in the course of the annual cycle.
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  • 7
    ISSN: 1570-7458
    Keywords: Diabrotica spp. ; corn rootworms ; Chrysomelidae ; Coleoptera ; plant-derived semiochemicals ; starch matrix ; encapsulation ; controlled release
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé Le programme expérimental de 1987 était destiné à déterminer: 1) si les substances dérivées de végétaux et attractives pour Diabrotica pouvaient être encapsulées dans de l'amidon additionné d'acide borique; 2) si différentes formules attireraient les différentes espèces de Diabrotica dans un champ de maïs. L'indol, l'estragol, le vératrol, le phénylacétaldéhyde et le trans-anéthol n'ont pas été retenus, tandis que le trans-cinnamaldéhyde, la \-ionone, le 1,2,4-triméthobenzène, l'eugénol et l'isœugénol ont été encapsulés avec succès dans des pièges attachés à des pieds de maïs (les détails techniques sont fournis). Les pièges ont été relevés tous les 4 jours du 11 juillet au 8 septembre. Les résultats montrent que les substances allélochimiques sont conservées dans la capsule pendant des durées variables et libérées à des concentrations attractives pour les Diabrotica adultes. Un mélange de trans-cinnamaldéhyde et de 1,2,4,-triméthoxybenzène a été la formule la plus efficace, à l'exception des périodes de formation des barbes et du pollen, où aucune formule n'a été attractive. Bien que la variation saisonnière des réactions de Diabrotica limite l'utilisation des substances allélochimiques d'origine végétale, la capsule d'amidon peut être employée pour libérer des substances allélochimiques et constitue un outil potentiel pour la mise au point d'une méthode plus rationnelle de lutte contre Diabrotica.
    Notes: Abstract The concept of encapsulating semiochemicals into a starch matrix is being studied for potential use in corn rootworm (CRW) management programs. During 1987, experiments were conducted to determine: 1) If volatile plant-derived Diabrotica spp. attractants could be encapsulated in a starch borate matrix (SBM), and 2) If various SBM-semiochemical formulations would attract Diabrotica species over time in field corn. Chemical analyses of fresh SBM formulations indicated that indole, estragole, veratrole, phenylacetaldehyde, and trans-anethole were not retained during formulation but trans-cinnamaldehyde, Beta-ionone, 1,2,4,-trimethoxybenzene, eugenol and isœugenol were successfully encapsulated. Encapsulated semiochemical formulations were made into 20 mesh granules, placed in Pherocon ® 1C traps that were tied to corn plants, and sampled for CRW adults every 4 days from 11 July to 8 September. Field data indicated that encapsulated semiochemicals were retained in the SBM for varying lengths of time and were released at rates attractive to CRW adults. A two-component mixture of trans-cinnamaldehyde and 1,2,4-trimethoxybenzene was the most effective formulation tested; however, no formulation was effective during corn silking and pollination. Although seasonal variation in CRW response could limit the usefulness of some plant-derived semiochemicals, the starch matrix concept may be useful as a delivery system for semiochemicals and may have potential as a tool that could be used in the development of new more biorational CRW management programs.
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  • 8
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    Entomologia experimentalis et applicata 50 (1989), S. 61-67 
    ISSN: 1570-7458
    Keywords: Coleoptera ; Chrysomelidae ; northern corn rootworm ; western corn rootworm ; dispersal ; malaise trap ; habitat selection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé Les activités de vol de D. barberi (NCR) et D. virgifera virgifera (WCR) ont été contrôlées par l'utilisation de pièges ‘malais’ placés en lisière de deux petits champs de maïs. Les populations de ces coléoptères sont maximales quand le maïs fleurit, mais leurs captures sont restées faibles jusqu'à ce que les barbes du maïs aient été sèches. Les captures de NCR et, dans une plus faible mesure, celles de WCR ont alors augmenté et sont restées importantes pendant toute la saison. Les pièges ‘malais’ ont été conçus pour que les adultes pénétrant par les côtés opposés soient récoltés séparément. Les femelles de NCR capturées face au champ de maïs avaient tendance à contenir moins d'ovocytes mûrs que celles capturées du côté opposé. Ces observations appuient l'hypothèse que les femelles NCR émigrent des champs de maïs pour s'alimenter, quand les barbes et le pollen de maïs, aliments préférés, deviennent indisponibles, mais que les femelles NCR pleines d'ovocytes mûrs recherchent le maïs quand elles sont en quête de lieux de ponte.
    Notes: Abstract Flight activity of corn rootworm beetles, the northern (NCR), Diabrotica barberi (Coleoptera: Chrysomelidae), and western (WCR), D. virgifera virgifera, was monitored using malaise traps placed at the edges of two small cornfields. Populations of beetles in the fields peaked while corn was flowering, but capture in malaise traps remained low until silks had dried. Capture of NCR and (to a lesser extent) WCR then increased and remained high through the season. Malaise traps were constructed to permit separate collections of beetles that entered on each of two opposite sides. Female NCR that were captured in sides that faced toward corn tended to contain fewer mature eggs than those in sides facing away from corn. These findings support the hypothesis that female NCR emigrate from cornfields to feed when fresh silk and corn pollen (favored foods) become unavailable, but that egg-laden NCR actively seek corn when searching for oviposition sites.
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  • 9
    ISSN: 1573-1561
    Keywords: Sweet potato weevil ; Cylas formicarius elegantulus ; Coleoptera ; Curculionidae ; Ipomoea batatas ; sweet potato volatiles ; sesquiterpenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract A dual-choice olfactometer was developed to study the responses of sweet potato weevils,Cylas formicarius elegantulus (Summers), to volatiles from the sweet potato,Ipomoea batatas (L.) Lam. Both males and females were attracted by volatiles from sweet potato leaves and a methylene chloride leaf extract. Females, but not males, responded to volatiles from storage roots and a methylene chloride root extract. Leaves and storage roots from four sweet potato cultivars (Centennial, Jewel, Resisto, and Regal) were attractive to female weevils; however, the attractant response varied with cultivar. GC profiles from leaf and root extracts, and GC-MS analysis of leaf extract, for Jewel cultivar enabled the volatile peaks to be identified as sesquiterpenes.
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  • 10
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    Journal of chemical ecology 15 (1989), S. 1729-1745 
    ISSN: 1573-1561
    Keywords: Kairomones ; host attraction ; monoterpenes ; ethanol synergism ; turpentine ; trapping ; Cerambycidae ; Scolytidae ; Curculionidae ; Cleridae ; Buprestidae ; Dryocetes autographus ; Monochamus scutellatus ; Hylobius pales ; Coleoptera
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Field experiments using baited sticky stovepipe traps and Lindgren multiple funnel traps were done near Chalk River, Ontario, Canada, to determine the effects of conifer monoterpenes (α-pinene, β-pinene, myrcene, limonene, camphene and carene) and ethanol on the number of beetles captured. Several species of conifer-feeding beetles were attracted to the monoterpenes or to monoterpenes and ethanol, including species in the families Cerambycidae (Asemum striatum, Acmaeops proteus, Xylotrechus undulatus, Monochamus scutellatus), Curculionidae (Pissodes strobi, Hylobius pales), and Scolytidae (Dryocetes autographus, Ips grandicollis). Species of Buprestidae generally did not respond to the monoterpenes or to ethanol. Species of Cleridae (Thanasimus dubius, Enoclerus nigripes rufiventris, Enoclerus nigrifrons gerhardi) which are predators of conifer bark beetles were attracted to the monoterpenes. Synergism between monoterpenes and ethanol was evident forM. scutellatus, H. pales, andD. autographus. While α-pinene was the most potent attractant for most beetle species, monoterpenes other than α-pinene synergized attraction to ethanol forD. autographus. Attraction of beetles to commercial turpentine and ethanol did not differ significantly from attraction to a pure monoterpene blend and ethanol.
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  • 11
    ISSN: 1573-1561
    Keywords: Defensive mechanism ; avoidance response ; Eumeces inexpectatus ; Pasimachus subsulcatus ; Coleoptera ; Carabidae ; lizard ecology ; lizard predation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The carabid beetlePasimachus subsulcatus is an abundant ground-dwelling insect in west central Florida that exudes a powerful mucous membrane irritant when disturbed. This secretion can be sprayed over 10 cm from the abdominal tip. The southeastern five-lined skink,Eumeces inexpectatus, is an abundant insectivorous lizard sympatric withPasimachus. We assessed the availability ofPasimachus toEumeces and found it to be within the foraging microenvironment of the lizard. Analysis ofEumeces gut contents and field feeding trials indicate thatPasimachus are not ingested by the lizard, yet arthropods of comparable size and exoskeletal thickness are ingested. The movement response ofEumeces to isolatedPasimachus secretion constituents, conducted in a modified Y-maze laboratory experiment, was used to assess the repellent capabilities of the secretion.Eumeces are consistently repelled byPasimachus secretion constituents, indicating that the beetle is protected chemically from the lizard.
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  • 12
    ISSN: 1573-1561
    Keywords: Synergism ; aggregation pheromone ; Pityogenes chalcographus ; Coleoptera ; Scolytidae ; chalcogran ; methyl (2E,4Z)-2,4-decadienoate ; enantiomers ; isomers ; stereoisomers ; synthesis ; bioassay ; structure-activity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Syntheses of all four Stereoisomers (2S,5S; 2S,5R;2R,5R; and2R,5S) of chalcogran, a major component of the aggregation pheromone ofPityogenes chalcographus, and of all four isomers (2Z,4Z; 2Z,4E; 2E,4E; and 2E,4Z) of methyl 2,4-decadienoate (MD), the second major pheromone component, are briefly described. Attraction responses of walking beetles of both sexes were tested to mixtures of the synergistic pheromone components or analogs. These bioassays showed that theE,Z isomer of MD is the most active when tested with chalcogran. When tested with (E,Z)-MD, (2S,5R)-chalcogran was the most active stereoisomer, while 2R,5R and 2R,5S isomers had intermediate activities, and the 2S,5S isomer was inactive. There was no evidence that the relatively less active Stereoisomers of chalcogran inhibited or promoted attraction to (2S,5R)-chalcogran with (E,Z)-MD. Male beetles only produce the activeE,Z isomer of MD (inactive alone) and their hindguts contain the most active (2S,5R)- and least active (2S,5S)-chalcogran. A mixture of all MD isomers with racemic chalcogran was not significantly different in attractivity compared to (E,Z)-MD with racemic chalcogran, indicating no synergistic or inhibitory effects of the inactive isomers of MD.
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  • 13
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    Journal of chemical ecology 15 (1989), S. 1837-1845 
    ISSN: 1573-1561
    Keywords: Defense ; deterrent ; sequestration ; iridoid glycoside ; paederoside ; Acyrthosiphon nipponicus ; Homoptera ; aphid ; Aphididae ; Harmonia axyridis ; Coleoptera ; Coccinellidae ; Paederia scandens
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract A Rubiaceae-feeding aphid,Acyrthosiphon nipponicus, is seldom attacked by the ladybird beetle,Harmonia axyridis. A potent deterrent against the beetle was isolated from the aphid and identified as paederoside, an iridoid glycoside originating in the aphid's host,Paederia scandens. The iridoid content was as high as 2% of the intact body weight, and a large portion was found in the cornicle secretion.
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  • 14
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    Journal of chemical ecology 15 (1989), S. 1015-1031 
    ISSN: 1573-1561
    Keywords: Saw-toothed grain beetle ; Oryzaephilus surinamensis ; Coleoptera ; Silvanidae ; aggregation pheromone ; electroantennogram ; behavioral bioassay ; blend ratio
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The antennal and behavioral responses of the saw-toothed grain beetle,Oryzaephilus surinamensis, to the three components of its male-produced aggregation pheromone were investigated. EAG recordings showed no differences between the responses of the two sexes to the synthetic pheromone components. In contrast, laboratory behavioral assays demonstrated marked differences between the sexes. More females than males were consistently attracted to mixtures of the synthetic components, and this bias appeared to be caused by one component in the blend. Altering the blend ratio resulted in changes in the ratio of the sexes attracted. Thus, if, as suggested by preliminary work, males vary the blend produced, this should alter the relative response of the sexes to the aggregation pheromone.
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  • 15
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    Journal of chemical ecology 15 (1989), S. 507-516 
    ISSN: 1573-1561
    Keywords: Monochamus alternatus Hope ; Coleoptera ; Cerambycidae ; pine inner bark ; methanol extracts ; water extracts ; oviposition stimulants ; lightwood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Field and laboratory ovipositional responses ofMonochamus alternatus Hope, respectively, to methanol and water extracts from pine inner bark were examined in comparison with those to pine inner bark, especially using a laboratory-built apparatus for the latter bioassay. Irrespective of the existence of volatiles from paraquat-induced lightwood, pine inner bark and its methanol and water extracts stimulated ovipositional response only in the presence of free moisture.
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  • 16
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    Journal of chemical ecology 15 (1989), S. 1147-1159 
    ISSN: 1573-1561
    Keywords: Ips paraconfusus ; bark beetles ; Coleoptera ; Scolytidae ; olfaction ; orientation ; anemotaxis ; pheromones
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Synthetic pheromone was released from a dispenser stretched across the width of a wind tunnel. Beetles in pheromone-free wind wandered in all directions and did not appear to orient to the wind. A dosage series showed that pheromone decreased the walking rate and deviations from the upwind direction, and it increased the turning rate. The tracks were composed of relatively straight or gently curving sections interspersed with more infrequent, larger course adjustments. Although pheromone clearly affected the average heading of beetles within a treatment, any given individual exposed to pheromone did not necessarily head directly upwind or maintain a fixed absolute angle with respect to the wind direction. The response appeared to be an inaccurate anemotaxis, rather than an anemomenotaxis.
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  • 17
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    Chromatographia 27 (1989), S. 27-30 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; 1,ω-Di(alkoxy)-polysulphides ; Retention contributions
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    Topics: Chemistry and Pharmacology
    Notes: Summary The reaction of S2Cl2 with alcohols yields products, the reversed-phase liquid chromatograms of which are similar to those of dialkyl-polysulphides RSnR, i.e., they represent homologous series. Four of the products were identified via GC-MS as 1,ω-di(alkoxy)-polysulphides having the general structure ROSnOR. Retention contributions of alkyl groups R and sulphur atoms in the −Sn — chain are not much different from values observed with polysulphides. The effect of oxygen, however, is only about −100 index units per O atom, while in dialkyl ethers values of −500 units have been reported.
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  • 18
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    Chromatographia 27 (1989), S. 5-14 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention behaviour ; Column parameters
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention of small molecules on reversed phase or other hydrophobic stationary phases can be represented by k′ values of members of a homologous series at varying solvent compositions. The evaluation of simple linear relationships leads to the introduction of a set of four parameters that contain all the information about retention behaviour of this homologous series in the binary solvent system chosen. It is possible to extrapolate to a hypothetical non-hydrophobic molecule and a solvent, the polarity of which equals that of the stationary phase, to characterize the properties of the stationary phase — eluent system. In addition, a chromatographic method for determination of the phase ratio of the column is proposed.
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  • 19
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion exchange separation ; Preparative separations ; Human chorionic gonadotropin hormone
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    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatography (HPLC) method was developed for the purification of 50mg crude human chorionic gonadotropin (HCG) hormone sample in one chromatographic run on a 250×10 mm SERVA DEAE Poliol-Si-500 column. During the 60-minute linear gradient of 0.05 M sodium sulfate, 0.05 M sodium hydrogen sulfate and 0.05% (v/v) acetonitrile in buffer “B” complete separation was accomplished in 40 min. Identity and purity of the fractions were checked by SDS electrophoretic method. The eluted HCG fractions were dialyzed for 24 hours to remove the buffer salts and liophilized. The activity of the hormone did not decreased significantly during the purification procedure.
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  • 20
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    Plant systematics and evolution 168 (1989), S. 1-5 
    ISSN: 1615-6110
    Keywords: Angiosperms ; Dilleniaceae ; Hibbertia hypericoides ; Mimosaceae ; Acacia ; Coleoptera ; Scarabaeidae ; Diphucephala ; Beetle/plant associations ; non-pollinator ofHibbertia ; potentialAcacia pollinator ; Flora of Australia
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    Topics: Biology
    Notes: Abstract Notes are provided on the association of the beetleDiphucephala affinis (Scarabaeidae) with yellow flowers ofHibbertia hypericoides, H. huegelii (Dilleniaceae),Acacia pulchella, andA. stenoptera (Mimosaceae). Observations were undertaken during September 9–19, 1979 at S. Perth, Western Australia. They indicated thatD. affinis is not a pollinator ofHibbertia as suggested in the literature, but may play a small role in the pollination of someAcacia species.
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  • 21
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    Journal of chemical ecology 15 (1989), S. 255-263 
    ISSN: 1573-1561
    Keywords: Monolepta beetle ; red-shouldered leaf beetle ; Monolepta australis ; lipid extract ; unsaturated aliphatic ethers ; 7-octadecenyl alkyl ethers ; gas chromatography-mass spectrometry ; Coleoptera ; Chrysomelidae
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Investigation of the lipid extract of the Australian chrysomelid beetle,Monolepta australis, has revealed a novel homologous series of long-chain, unsaturated-saturated dialkyl ethers in the cuticular wax. Gas chromatography-mass spectrometry, proton magnetic resonance, infrared spectroscopy, and chemical degradation have shown that ethers of formula CH3(CH2)9CH=CH(CH2)6O(CH2)12–16CH3 predominate.
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  • 22
    ISSN: 1573-1561
    Keywords: Ips pini ; Coleoptera ; Scolytidae ; aggregation pheromone ; ipsdienol ; geographic variation ; intrapopulation variation ; speciation
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract We determined the chirality of ipsdienol in individual male pine engravers,Ips pini (Say), from New York, California, and two localities in British Columbia (BC). Both quantity and chirality of ipsdienol varied significantly between and within populations ofI. pini. Beetles from California and southeastern BC produced primarily (R)-(−)-ipsdienol with mean ratios of (S)-(+) : (R)-(−) of 9 : 91 and 11 : 89, respectively, while beetles from New York produced primarily (S)-(+)-ipsdienol with a mean (S)-(+) : (R)-(−) ratio of 57 : 43. A population from southwestern BC was unlike any other known western population, producing primarily (S)-(+)-ipsdienol with a mean (S)-(+) : (R)-(−) ratio of 66 : 34. In contrast to the unimodal chirality profiles for ipsdienol production in populations from California and southeastern BC, the profiles of the populations from southwestern BC and New York were bimodal, with a common mode at approximately 44 : 56 (S)-(+) : (R)-(−). Bimodality in the profiles of ipsdienol chirality in two populations ofI. pini and remarkably high levels of intrapopulation variation in pheromone chirality in all four populations suggest that evolutionary change in pheromone channels of communication could occur, possibly in response to artificial selection pressures such as mass trapping.
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  • 23
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    Journal of chemical ecology 15 (1989), S. 807-817 
    ISSN: 1573-1561
    Keywords: Coleoptera ; Scolytidae ; Tomicus piniperda ; Trypodendron lineatum ; Hylurgops palliatus ; Thanasimus formicarius ; host attraction ; host volatiles ; ethanol ; α-pinene ; synergism
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The attraction of bark and ambrosia beetles as well as associated beetles to α-pinene and ethanol was studied in field experiments with flight barrier traps. α-Pinene and ethanol were released individually and as combinations in approximately 1∶1 or 1∶10 ratios and at four different release rates. Ethanol attractedTomicus piniperda (L.),Hylurgops palliatus (Gyll.),Trypodendron lineatum (Oliv.),Hylastes cunicularius Er.,H. brunneus Er.,H. opacus Er., andAnisandrus dispar (F.) (Scolytidae);Glischrochilus quadripunctatus (L.) andEpuraea spp. (Nitidulidae);Thanasimus formicarius (L.) (Cleridae); andRhizophagus depressus (F.) (Rhizophagidae). α-Pinene attracted all these species with the exception ofT. lineatum, H. cunicularius, andA. dispar. Combinations of a-pinene and ethanol resulted in synergistically increased attraction of all species with the exception ofH. opacus andA. dispar. A. dispar, the only hardwood-associated species in the study, was repelled by α-pinene. Both the release rates and the ratio at which the two substances were released influenced the response of the beetles. The differences in response between the beetle species seem to reflect dissimilarities in the release of the two substances among the various types of breeding material to which the species are adapted.
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  • 24
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    Journal of chemical ecology 15 (1989), S. 3-24 
    ISSN: 1573-1561
    Keywords: Ips paraconfusus ; Coleoptera ; Scolytidae ; bark beetles ; taxis ; chemotaxis ; orientation ; olfaction ; pheromones
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Gas-liquid chromatography of the air within the arena developed for this assay showed that a concentration gradient was established within 1–2 min of applying the pheromone (ipsenol, ipsdienol,cis-verbenol), and that this gradient was nearly constant for 20–95 min after application. The concentration fell rapidly and approximately exponentially between the source and the center of the arena. Turning rate and the number of beetles that reached the source increased, and heading with respect to the source decreased, in the presence of pheromone. Responses of beetles that did and did not reach the source were significantly different, but within each group there were no significant differences among dosages. Turning rate and heading varied little with distance from the source, while walking rate decreased as distance from the release point of the beetles increased. We hypothesize that dosage exerts its major effect on source location by altering the probability that a beetle will enter into orientation behavior and that beetles orienting to sources have similar behaviors even when orienting to a wide range of dosages.
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  • 25
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    Journal of chemical ecology 15 (1989), S. 183-208 
    ISSN: 1573-1561
    Keywords: Ips paraconfusus ; Coleoptera ; Scolytidae ; bark beetles ; olfaction ; orientation ; counterturning ; chemotaxis ; taxis ; pheromones ; tropotaxis ; schemakinesis
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The position of beetles were marked at 1-sec intervals after they were released in still air 16–18 cm from point sources of pheromone. Characteristics of the tracks were quantified and compared to those that might be produced by counterturning schemakinesis, tropotaxis, klinotaxis, zigzagging, look-and-leap, or steepest-ascent schemakinesis mechanisms. The beetles' movements were highly irregular, but they turned almost continually and never fixed on a heading near 0° (=straight towards the source). Turn angle sizes increased slightly with absolute size of heading but had the opposite sign, thus compensating slightly for heading. Their distribution was centered about 0° and was unimodal. Heading decreased gradually as the source was neared, but the decrease became steeper within 1–5 cm of the source. Histograms showed that the maximum headings between occurrences when the beetle was headed directly towards the source (0°) were centered around 0° and most of them were less than 90°. However, maximum headings between 90° and 180° were not uncommon. Turn radius decreased as the source was neared. The counterturning mechanism was the most consistent with these observations. An analysis of rate of change of concentration with respect to heading and distance to the source further demonstrated that the counterturning mechanism could explain the form of the decrease in heading as the source was neared, if the major cue used to initiate counterturns was a decrease in the rate of increase of concentration. The tropotaxis could not recreate the form of the decrease, under any form of stimulus processing.
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  • 26
    ISSN: 1573-1561
    Keywords: Ips typographus ; Coleoptera ; Scolytidae ; Picea abies ; aggregation pheromones ; host tree resistance ; tree-switching ; GC-MS ; monoterpenes ; 2-methyl-3-buten-2-ol ; cis-verbenol, verbenone
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Volatiles released from individual entrance holes of eight spruce bark beetles (Ips typographus) were collected during the first week of attack on a resistant host tree. In order to quantify the release of the highly volatile 2-methyl-3-buten-2-ol (MB) from attacking males, a new method was developed with deuterated quantification standard released at the time of collection. The amounts of collected volatiles, as analyzed by GC and GC-MS, showed a large variation between individual holes and also between subsequent entrainments from the same hole. Most of the quantified compounds on the average have two maxima, with a pronounced intervening depression. The amounts of releasedcis-verbenol (cV) increased five times during the first two days, while the amounts of MB were consistently high. The attacked spruce tree was not taken by the beetles, and the average amounts of the two aggregation pheromone components, MB and cV, increased again after the first maxima. The first peak of oxygenated monoterpene, released in the beginning of the attack containing α-terpineol, terpinen-4-ol, bornyl acetate,trans-pinocarveol, and verbenone, was possibly due to spontaneous oxidation of monoterpene hydrocarbons from the tree. Microorganisms established in the gallery wall phloem probably participated in the production of oxygenated monoterpenes during the second increase.
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  • 27
    ISSN: 1573-1561
    Keywords: Boll weevil ; olfaction ; receptor cell ; Anthonomus grandis ; Coleoptera ; Curculionidae ; enantiomer ; grandisol ; chirality ; electroantennogram ; aggregation pheromone ; neurobiology ; structure-activity
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Electrophysiological recordings from antennal olfactory receptors and field behavioral experiments showed both male and female boll weevils,Anthonomus grandis Boh. (Coleoptera: Curculionidae), to respond specifically to (+)-grandisol, an enantiomer of compound I of the boll weevil aggregation pheromone. Single-cell recordings revealed antennal olfactory neurons in both male and female weevils keyed to (+)-grandisol. Electroantennograms in response to serial dilutions of the grandisol enaniiomers showed a threshold 100 to 1000 times lower for (+)-grandisol relative to its antipode. In field behavioral experiments, both sexes were significantly more attracted to (+)-grandisol in combination with the three other pheromone components than the combination with (−)-grandisol. When (−)-grandisol was placed with the (+)-enantiomer at equal dosages, a slight although statistically insignificant inhibition occurred. Subsequent field tests showed that the low level of attraction exhibited by (−)-grandisol in combination with the other three pheromone components could be attributed to the other three components alone. These results are in contrast with an earlier study, which found (−)-grandisol to be as attractive as the (+)-enantiomer.
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  • 28
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    Journal of chemical ecology 15 (1989), S. 767-777 
    ISSN: 1573-1561
    Keywords: Anthonomus grandis ; behavior ; boll weevil ; Coleoptera ; cotton ; cultivar ; Curculionidae ; effluvial method ; grandlure ; pheromone ; Pora-pak Q ; pheromone collection ; aeration collection
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract An effluvial method was developed to collect the pheromone, grandlure from actively calling male boll weevils,Anthonomus grandis Boheman. The adsorbant, Porapak Q (ethylvinylbenzene-divinylbenzene), was utilized to trap and concentrate the pheromone. Captured pheromone was desorbed from columns packed with Porapak Q by elution withn-pentane and quantified by capillary column gas-liquid chromatography. In recovery studies with known amounts of synthetic grandlure, we found that the amount of each pheromone component collected was a function of collection duration, elution volume, and initial concentration. This effluvial method was capable of recovering as much as 94.9% of a known quantity (80 μg) of grandlure. The chromatograms were free of extraneous peaks. In studies of insect-produced pheromone, the effluvial method was used to collect pheromone from the air space surrounding male boll weevils as they fed on flower buds from CAMD-E cotton. The quantity and quality of boll-weevil-produced pheromone was determined for days 6, 8, 10, 11, 12, 13, and 14 of boll weevil adulthood. The maximum quantity of natural pheromone was produced on day 13 (4.2 μg/weevil) with a pheromone component ratio of 2.41∶2.29∶0.95∶1 for components I, II, III, and IV, respectively. The effluvial method described in this report is an efficient method to collect and quantify boll weevil pheromone from the atmosphere surrounding actively calling insects. Other applications of this method are suggested.
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  • 29
    ISSN: 1573-1561
    Keywords: Boll weevil ; Anthonomus grandis ; aggregation pheromone ; multicomponent ; behavior ; electroantennogram ; neurobiology ; structureactivity ; geometric isomers ; cotton ; Coleoptera ; Curculionidae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract For two decades, the aggregation pheromone of the boll weevil,Anthonomus grandis Boh. (Coleoptera: Curculionidae), was thought to consist of four compounds: I [(+)-(Z)-2-isopropenyl-1-methylcyclobutane ethanol]; II [(Z)-3,3-dimethyl-ΔI,β-cyclohexane ethanol]; III [(Z)-3,3-dimethyl-Δ1,α-cyclohexane acetaldehyde); and IV [(E)-3,3-dimethyl-Δ1,α-cyclohexane acetaldehyde). Evidence is presented from behavioral and electrophysiological studies to show that only three of these components, I, II, and IV, are essential for attraction. Competitive field tests, in which each possible three-component blend was tested against the four-component mixture, demonstrated that omission of I, II. or IV resulted in decreased trap captures (P 〈 0.01). Trap captures by these blends lacking I, II, or IV resembled those by the hexane solvent alone in a similar experiment. However, omission of III did not significantly alter field attractiveness of the blend. Dosage-response curves constructed from electroantennogram responses of both males and females to serial dilutions of III, IV, and a 50∶50 mixture of the geometric isomers III and IV showed both sexes to be 10- to 100-fold more sensitive to IV than III. Data from the electrophysiological studies were consistent with a single acceptor type for the (E)-cyclohexylidene aldehyde, IV, for males, and possibly one or two acceptor types for III and IV for females. Possible roles for the (Z)-cyclohexylidene aldehyde, III, and implications for the pheromonal attractant currently used in boll weevil eradication/suppression programs are discussed.
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  • 30
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    Journal of chemical ecology 15 (1989), S. 2263-2277 
    ISSN: 1573-1561
    Keywords: Aggregation pheromone ; Ips typogmphus ; Coleoptera ; Scolytidae ; density regulation ; inhibitor ; verbenone ; ipsenol ; ipsdienol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The semiochemicals verbenone (Vn), ipsenol (Ie), and ipsdienol (Id), present in late phases of host colonization, have been implicated as qualitative “shut-off” signals regulating attack density. Combinations of the three chemicals were released in pipe traps together with the aggregation pheromone components 2-methyl-3-buten-2-ol (MB) andcis-verbenol (cV) at different levels and in different ratios to MB + cV, and with two spacings of traps to test for possible effects on reducing catch at traps baited with aggregation pheromone. When they were released with the attractants Vn and Ie (alone or together) decreased the mean catch significantly at the higher release rates used (1 mg/day). Id alone or together with Vn at low release rates (0.1 mg/day), with the attractants, increased catch somewhat. A dose-response test of Vn, with the attractants held constant, showed a decline in catches, down to about 〈 10% of the control, at ratios of Vn to cV between 1∶1 and 150∶ 1. A larger spacing (25 m) of traps gave a stronger response to change in doses of Vn and MB + cV than a smaller (6 m) spacing. The sex ratio was more skewed towards females when two or three inhibitors were present and at higher doses of Vn. It is suggested that Vn could be the most important density-regulating signal in the natural system, as release of Vn from galleries is larger and starts earlier than that of Id and Ie.
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  • 31
    ISSN: 1573-1561
    Keywords: Dendroctonus ponderosae ; Ips paraconfusus ; Coleoptera ; Scolytidae ; pheromones ; terpene alcohols ; axenic-rearing ; bark beetles ; microorganisms
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Dendroctonus ponderosae Hopkins andIps paraconfusus Lanier of both sexes produced most of their complement of terpene alcohols at normal to elevated levels in the absence of readily culturable microorganisms. However, there was some evidence that microbial involvement may be required by maleI. paraconfusus to produce ipsenol and ipsdienol at normal levels. Increased levels of certain terpene alcohols found in axenically reared or streptomycin-fed beetles suggest that symbiotic microorganisms may be responsible for breaking down pheromones and other terpene alcohols. There was also evidence for microbial involvement in the production of the antiaggregation pheromone verbenone inD. ponderosae. This compound was not produced in quantifiable levels by axenically reared or streptomycin-fed beetles exposed to α-pinene as vapors or through feeding, but was found in wildD. ponderosae exposed to α-pinene through feeding on bolts of lodgepole pine,Pinus contorta var.latifolia Engelmann.
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  • 32
    ISSN: 1573-1561
    Keywords: Dendroctonus terebrans ; Coleoptera ; Scolytidae ; bark beetles ; pheromones ; primary attraction ; secondary attraction ; host selection ; frontalin ; exo-brevicomin
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    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Controlled infestation ofDendroctonus terebrans (Olivier) on bolts of slash pine,Pinus ellionii Engelm. var.elliottii, elicited greater attraction of wild conspecifics than uninfested bolts. Secondary attraction was not apparent, however, to standing slash pines that had received volunteer attacks, when compared with attraction to unattacked but susceptible trees. Hindguts from in-flight or attacking femaleD. terebrans contained frontalin, and those from in-flight or attacking males containedexo-brevicomin.Trans-pinocarveol,cis-verbenol,trans-verbenol, myrtenal, verbenone, myrtenol, and other compounds were produced by both sexes during gallery construction in host trees. Synthetic frontalin, when deployed with a standard host odor mixture of turpentine and ethanol, was very attractive to maleD. terebrans in field-trapping experiments. The addition of eitherexo-brevicomin orendo-brevicomin to the frontalin-turpentine combination negated the attractive effect of frontalin for males.Trans-verbenol, myrtenol, and verbenone had little effect onD. terebrans behavior. Responses of females did not differ among treatments in any of the 11 field experiments.
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  • 33
    ISSN: 1573-1561
    Keywords: Olfaction ; chirality ; pheromone ; semiochemical ; enantiomer ; bark beetle ; electrophysiology ; electroantennogram ; mountain pine beetle ; Dendroctonus ponderosae ; Coleoptera ; Scolytidae
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    Notes: Abstract Electroantennograms (EAGs) were recorded fromD. ponderosae to the enantiomers of the terpenoid bark-beetle pheromonestrans-verbenol,cis-verbenol, verbenone, and the bicyclic ketals frontalin,exo-brevicomin, andendo-brevicomin. Male and female responses to enantiomers of the terpenoids differed significantly only at the two highest concentrations. No sex differences were seen in response to the bicyclic ketals. Significantly different responses to the enantiomers of all the chemicals, except frontalin, were noted over at least part of the dosage-response ranges tested. The negative antipode for all of the terpenoids elicited higher responses, while for the bicyclic ketals, the positive antipode effected the largest responses except for the two highest concentrations ofexo-brevicomin.
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    Journal of comparative physiology 159 (1989), S. 589-596 
    ISSN: 1432-136X
    Keywords: Corpora cardiaca ; Coleoptera ; Neuropeptides ; HPLC ; Amino acid composition
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    Topics: Biology , Medicine
    Notes: Summary Extracts of corpora cardiaca from two members of the family Tenebrionidae,Zophobas rugipes andTenebrio molitor, from one member of the Chrysomelidae,Leptinotarsa decemlineata, and from three members of the Scarabaeidae,Pachnoda marginata, P. sinuata andMelolontha hippocastani, were assayed for adipokinetic and hypertrehalosaemic activity in acceptor locusts (Locusta migratoria) and cockroaches (Periplaneta americana), respectively. All corpus cardiacum material tested, except that from the cockchafer,M. hippocastani, gave positive bioassay results. Biological activities of corpus cardiacum extracts from all species investigated can be resolved on reversed-phase high performance liquid chromatography (RP-HPLC). Gland extracts from the two tenebrionid species each show a single peak of biological activity associated with a single peak of UV absorbance having an identical retention time in both species. The two biologically active fractions from the corpora cardiaca of the potato beetle,L. decemlineata, coelute with exogenous (synthetic) hypertrehalosaemic hormones I and II of the American cockroach. The two species of the genusPachnoda contain two active compounds in their glands; compound I of each species is more abundant and elutes just ahead of the (synthetic) hypertrehalosaemic hormone of the cockroachBlaberus discoidalis. The gland material ofM. hippocastani exhibits and absorbance peak with the same retention time as the major peak from thePachnoda-species; however, this peak material does not elicit biological activity in the assays used here. After fractionation by RP-HPLC the main biologically active compounds were subjected to amino acid analyses. All factors are peptidic and contain 8 amino acid residues. The peptides from the tenebrionid species have the amino acid residues Asx(2), Glx(1), Ser(1), Pro(1), Leu(1), Phe(1) and Trp(i), whereas the main peptide from corpora cardiaca ofP. marginata contains the residues Asx(2), Glx(1), Ser(1), Pro(1), Tyr(1), Leu(1) and Trp(1). Amino acid composition analyses of the two active fractions fromL. decemlineata reveal the residues Asx(2), Glx(1), Ser(1), Pro(1), Val(1), Phe(1) and Trp(1) for compound I and Asx(1), Glx(1), Thr(2), Pro(1), Leu(1), Phe(1) and Trp(1) for compound II.
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  • 35
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microcrystalline cellulose triacetate ; Molecular modeling ; Computer graphics
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    Topics: Chemistry and Pharmacology
    Notes: Summary Molecular modeling and energy calculations have been used to study the chromatographic separation of aromatic compounds on microcrystalline cellubose triacetate. A linear relationship has been found between the logarithms of the capacity factors and the energy values of the interaction of these compounds with this stationary phase. The interaction energies have been calculated for two different spatial dispositions of the solutes in relation to the sorbent.
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  • 36
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Liquid crystals ; Synthesis of new bonded phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary A compound which becomes a liquid crystal when bonded to a polysiloxane was reacted with dimethylchlorosilane to produce a reagent suitable for bonding to a silica surface. After the silanization reaction was complete, the product was characterized by elemental analysis, diffuse reflectance Fourier transform Infrared Spectroscopy (DRIFT), CP/MAS carbon-13 NMR and differential scanning calorimetry (DSC). Preliminary chromatographic testing was done by retention index measurements using the alkylarylketone homologous series and by measuring the separation factor, α, for anthracene/phenanthrene at two different mobile phase compositions.
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  • 37
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    Chromatographia 27 (1989), S. 633-638 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adsorption isotherms ; Equilibria criteria ; Silica and carbon adsorbents ; Aromatic compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Examples of high-performance liquid chromatography (HPLC) are given for the determination of adsorption equilibrium and distribution coefficients, calculation of excess adsorption isotherms from solutions ranging from 10−7 to 10−1 mole fraction, changes in activity coefficient of the component predominantly adsorbed from solution and substitution enthalpy. These examples stem from studies of HPLC and the static adsorption of benzene, anisole and benzaldehyde from solutions in n-heptane on macroporous silica and active carbon at various temperatures. A criterion is suggested for evaluating equilibrium in the HPLC process. The potential of size-exclusion chromatography (SEC) for evaluating the volume and predominant diameter of adsorbed pores as well as pore diffraction are discussed. Prospects for HPLC application to molecularstructural analysis and other purposes are discussed briefly.
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  • 38
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    Chromatographia 27 (1989), S. 118-122 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase chromatography ; Non-aqueous reversed-phase chromatography ; Polycyclic aromatic hydrocarbons ; Solvent strength
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    Topics: Chemistry and Pharmacology
    Notes: Summary Elution strengths of 11 common HPLC solvents on a polymeric C18 phase were compared using a marker set of polycyclic aromatic hydrocarbons. Naphthalene, pyrene, benzo[ghi]perylene, and three larger naphthologues of 8, 10, and 12 rings (constituting a “naphthalene zigzag” series) were chosen because they span the solvent strength range up to and including the strongest solvents, tetrahydrofuran (THF) and chlorobenzene. Four pairs of similarly shaped isomers were used to probe solvent selectivity. With the exception of THF, HPLC solvent strength correlated with observed red shifts of fluorescence band maxima in each solvent. For THF, the pure solvent and blended mixtures behaved quite differently.
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  • 39
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    Chromatographia 27 (1989), S. 156-158 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mobile phase retention time ; Capacity factor ; Negative capacity factor
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    Topics: Chemistry and Pharmacology
    Notes: Summary Numerous ideas and procedures have been suggested in the literature for the determination of tm, the retention time of a non-retained species, in high-performance liquid chromatography. In some cases chromatograms have been obtained showing sample components eluting prior to the assumed non-retained species. This phenomenon results in apparent negative capacity factors for the species in question. We have proposed a method employing small inorganic anions which results in a limiting value for tm and eliminates apparent negative capacity factors.
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  • 40
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    Chromatographia 27 (1989), S. 228-232 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase ; 13C n.m.r. ; Arginine-aldehyde peptides ; GYKI-14166
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    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatographic and13C n.m.r. spectrometry methods were used for the investigation of peptides containing arginine-aldehyde moiety. Investigation of a model compound, N-benzoyl-Arg-H, showed that in an acidic mobile phase peptides containing the arginine-aldehyde group elute in three characteristic peaks. The components of the peaks were found to be constituents of an equilibrium mixture. The structures of the two components were identified, one as the aldehyde hydrate, the other as the cyclanol derivative. The reactivity of TRIS (HCl) buffer at pH 8.5 with the arginine aldehyde moiety was used for the assignment of the equilibrium structures.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase ; Ion-pair ; Recoveries ; Hepatocytes ; Purine compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Three groups of metabolites were analyzed in extracts of rat hepatocytes by an HPLC method: (i) nucleotides (ATP, ADP, AMP, GTP, GDP, UTP, UDP, IMP, UMP), (ii) nucleosides and nucleobases (adenosine, adenine, guanosine, inosine, xanthine, hypoxanthine, uridine) and (iii) inhibitors of xanthine oxidoreductase (oxypurinol, allopurinol). Perchloric acid extracts were neutralized with K2CO3/triethanolamine and analyzed at 254 nm by reversed-phase ion-pair high-performance liquid chromatography. The nucleotides and their derivatives were separated with a gradient elution using 10 mM NH4H2PO4/2 mM t-butylammonium-phosphate and acetonitrile. Recovery values were estimated for the extraction procedure used. The method was applied to the investigation of nucleotide metabolism of hepatocytes of starved rats at anoxia and reoxygenation.
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  • 42
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    Chromatographia 27 (1989), S. 316-320 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; Silica-based cation-exchanger ; Trimethylsilyl chlorosulfonate ; Lanthanides
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    Topics: Chemistry and Pharmacology
    Notes: Summary A low exchange-capacity, silica-based cation-exchanger for use in ion chromatography has been synthesized. (p-Trimethylsilyl)benzyl-dimethylchlorosilane (TBDCS) reacts with trimethylsilyl chlorosulfonate (TMCS) to produce a compound sulfonated in the para position of the type ArSO2OSi (CH3)3, which is bonded to 5 μm porous silica beads and hydrolysed to the corresponding arylsulfonic acid. The product is hydrophilic and has a high degree of sulfonation, efficiencies of packed columns reaching about 40,000–50,000 plates per meter for the separation of the Mn2+ ion. The new stationary phase has been applied to the ion chromatography of some organic and inorganic ions. It is notable that 14 lanthanides can be separated by isocratic elution about one hour on a 150×4·6 mm column, with 4 mM ethylenediamine and 6 mM α-hydroxyl-isobutanoic acid (pH 3.67) as mobile phase.
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  • 43
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    Chromatographia 27 (1989), S. 191-193 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Dansyl amino acids ; Chemiluminescence ; Bis(2,4,6-Trichlorophenyl)oxalate, (TCPO) ; Enhancement of luminescence
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    Topics: Chemistry and Pharmacology
    Notes: Summary The dansylated amino acids alanine, glutamic acid, methionine and norleucine were separated by reversedphase HPLC and detected via chemical excitation using the post-column, TCPO-peroxyoxalate reaction system. Enhancement of the chemiluminescence emission was achieved by including the surfactant Triton X-100 in the eluent.
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  • 44
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reverse-phase chromatography ; Elastin Hydrolysis measurement ; On-line post-column derivatization
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    Topics: Chemistry and Pharmacology
    Notes: Summary Excessive breakdown of elastin, a structural protein, may be related to aortic disease and emphysema. Since L-valyl-L-proline occurs in high concentrations in elastin, a rapid and sensitive method using HPLC with post-column on-line derivatization was used to measure the dipeptide from swine aortic tissue, and the amount of elastin present was determined. Elastin was extracted by alkaline hydrolysis. After neutralization and filtration, the sample was injected onto a ODS-2 gel column, and the dipeptide was eluted by a linear gradient of 0 to 10% of 1-propanol in 50 mM heptafluorobutyrate, pH 3, at a flow rate of 1 ml/min. The eluent was reacted with fluorescamine at pH 8.6, and fluorescence was detected at an excitation wavelength of 395 nm and a 455 nm cutoff emission filter.
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  • 45
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    Chromatographia 27 (1989), S. 449-454 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion exchange and affinity columns in series ; Porcine pancreatic enzymes ; Trypsin and elastase
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    Topics: Chemistry and Pharmacology
    Notes: Summary In order to separate and purify some of the enzymes contained in porcine pancreas, operation of an ion-exchange column in series with an affinity column has been used. The enzymes dealt with possess very similar molecular weights, isoelectric points and active sites. Hence they are difficult to separate and purify by traditional separation and/or purification methods. CM-Sepharose anion-exchange resin adsorbs elastase and trypsin at low pH (4.5) and desorbs them at high pH (9.0) and high ionic strength. Chitin-CHOM affinity adsorbent adsorbs trypsin at high pH (8.0) and desorbs it at low pH (2.5). By virtue of this complementary relationship two chromatographic columns were connected in series for facilitating the separation and purification of elastase and trypsin from porcine pancreas. The result showed that the specific activities of elastase and trypsin had been increased 16 and 22 fold respectively.
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  • 46
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    Chromatographia 27 (1989), S. 472-474 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hydrous titanium oxide ; Anion exchange ; Polyvalent anions
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    Topics: Chemistry and Pharmacology
    Notes: Summary Hydrous titanium oxide (HTiO), prepared under varying conditions of precipitation, has been studied for its anion exchange behaviour. Its chemical and thermal stability has been examined. The stoichiometry of uptake for Cl− has been investigated using a36Cl radiotracer and the regeneration power of the exchanger checked. Distribution coefficients for halides and polyvalent anions have been determined and on the basis of sorption data some polyvalent anions have been separated using HTiO columns.
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  • 47
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    Chromatographia 27 (1989), S. 509-512 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flavonoids ; Crataegus ; Passiflora ; Matricaria ; Ginkgo
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    Topics: Chemistry and Pharmacology
    Notes: Summary Flavonoids of Crataegus monogyna, Passiflora incarnata, Matricaria chamomilla and Ginkgo biloba extracts have been separated by isocratic elution on C18 columns using eluents based on C3 alcohols, tetrahydrofuran or dioxane. Satisfactory results have been obtained at compared to the low resolution achieved with the customary system acetonitrile-water-acetic acid.
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  • 48
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    Chromatographia 28 (1989), S. 19-23 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Preparation of stationary phases ; Polymer coated stationary phases ; Polymer-octyl bonded phase
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    Topics: Chemistry and Pharmacology
    Notes: Summary Polymethyloctylsiloxane-coated stationary phases have been prepared for liquid chromatography, by thermal reaction. The influence of the reaction conditions on retention and efficiency of test substances with different structures has been discussed. The materials have good stability in both acidic and basic eluents.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size exclusion ; Vesicular packing material ; Proteins and polymers
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new vesicular packing material — prepared from plant cell clusters by purification of the intact cell wall framework —is suitable for chromatography, giving high performance at low pressure gradients. The separation is achieved by dialysis through the cell wall, which is an ultrafilter membrane with an extremely sharp size limit of separation. Almost the whole of the stationary liquid phase is located within the vesicle (empty cell) lumina. In contrast to gel filtration vesicle chromatography gives a practically ideal separation of two size groups with an extremely short fractionation range. The size limit of separation was investigated by chromatography of proteins and other polymers. Group separation of molecules of a polydisperse dextran standard preparation showed that the critical Stokes' diameter for dextran permeation into the stationary liquid phase of the vesicular packing is 5 to 6 nm.
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  • 50
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Preparative scale separation ; 1,1-Dimethylethyl 4- and 5-bromo-trans-2-methylcyclohexane-1-carboxylate ; Trimedlure-related isomers ; Ceratitis capitata
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    Topics: Chemistry and Pharmacology
    Notes: Summary A semi-preparative high-performance liquid chromatographic procedure on 5-μm silica was developed for the isolation of gram quantities of four 1,1-dimethylethyl 4- and 5-bromo-trans-2-methylcyclohexane-1-carboxylate isomers (trimedlure-related) for NMR studies and comparative biological evaluation as male medfly,Ceratitis capitata, attractants.
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  • 51
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrochemical detection ; Pseudouridine ; Creatinine ; Urine analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The anodic behaviour of pseudouridine a modified nucleoside proposed as tumoral marker, has been studied at a mercury electrode. A method for its determination in urine samples by liquid chromatography with indirect anodic polarographic detection has been developed. The method is simple, highly selective and permits the direct injection of urine after dilution (1∶20) with mobile phase. Creatinine, which also gave an anodic response on mercury, could be simultaneously determined and used as an “internal standard” for Psi. This allowed the pseudouridine/creatinine ratio determination in a single run on the same specimen and the use of urine samples collected randomly instead of the 24h collection. The within-day RSD% for pseudouridine/ creatinine peak areas ratio was 3.4%.
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  • 52
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    Chromatographia 28 (1989), S. 9-14 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ester silicate silica gels ; Behaviour with organic bases ; Silanol groups ; Acidic centres
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    Topics: Chemistry and Pharmacology
    Notes: Summary Silica gels produced from ester silicates (ES-gels) are excellent chromatographic supports. In comparison with other silica gels the RP-materials obtained from them show little peak tailing even with polar, and, in particular, with basic compounds. Gels produced by various manufacturing processes have been classified by adsorption with methyl pyridinium chloride. ES-gels yield very low methyl pyridinium chloride values and small asymmetry parameters. The results indicate that there are strongly acidic, structurally-related surface centres which cause peak tailing on most commercial gels. It was shown that surface silanols on silica gels do not, in themselves, lead to peak tailing.
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  • 53
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    Chromatographia 28 (1989), S. 34-38 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Methylisothiazolones ; Preservatives ; Analysis of cosmetics
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    Topics: Chemistry and Pharmacology
    Notes: Summary Antimicrobially active formulations based on 2-methyl-3(2H)-isothiazolone and 5-chloro-2-methyl-3(2H)-isothiazolone (Kathon CG, Euxyl K 100) are incorporated into manufactured cosmetics as preservatives. In this paper we report on the analysis of these active components by means of liquid chromatography. It is conventional for the original methylisothiazolone components in cosmetics to be analyzed by reversed phase high-performance liquid chromatography after column chromatographic separation and flash chromatographic purification. In our new analytical method the methylisothiazolones are converted into the respective β-thiosubstituted acrylamide derivatives, which are ionic substances, with the help of the nucleophilic reagent hydrogensulfite. An ion pair high-performance liquid chromatographic method has been developed for the separation and quantification of these derivatives.
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  • 54
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oxygen radicals ; Nucleotides ; Aldehydes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The analysis of two metabolite groups, nucleotides and aldehydes, is necessary for assessment of oxygen radical metabolism during hypoxia and reoxygenation. Nucleotides and their derivatives were determined by HPLC using gradient elution with 10 mM NH4H2PO4 buffer containing 2 mM t-butylammoniumphosphate and acetonitrile. Aldehydes occuring after lipid peroxidation were analyzed by derivatisation to dinitrophenylhydrazones followed by TLC and HPLC separation with methanol/water on an ODS column.
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  • 55
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    Chromatographia 28 (1989), S. 209-211 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Triazine herbicides
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    Topics: Chemistry and Pharmacology
    Notes: Summary A number of 11 triazine herbicides and 7 of their corresponding metabolites were separated in a single HPLC run. The separation was achieved on a reversed-phase column using gradient elution with acetonitrile/buffer. Detection was by UV absorption at a wave-length of 220 nm.
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  • 56
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Polycyclic aromatic hydrocarbons ; Diode array and fluorescence detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary Both the separation of polycyclic aromatic hydrocarbons (PAH's) on tailor made HPLC phases, and their chromatographic enrichment and quantitative determination are of great interest. Because of the generally low concentrations of PAH's in the environment, and the low limiting values in German legislation for drinking water, methods for selective enrichment and sensitive detection are indispensable. On account of their relatively high amounts in soil, the determination of PAH's is valuable for the assessment of the potential danger to ground water by waste materials. These requirements can be fulfilled by used of solid phase extraction on enrichment columns, and fluorescence or UV/VIS diode array detection. For the detection of PAH's in the picogram range, the wavelengths for excitation and emission were time programmed over the chromatogram. With this feature, it is possible to detect all the individual compounds at the highest sensitivity, over the entire analysis.
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  • 57
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    Chromatographia 28 (1989), S. 289-292 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micro-bore and capillary columns ; Gradient techniques
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gradient delivery system for microbore and open tubular liquid chromatography is described. A gradient mixing vessel of 5–100μl, or 25–1000μl allows the generation of binary gradients with high reproducibility. The suitability of the system for short packed micro bore columns and open tubular columns is demonstrated.
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  • 58
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flecainide in plasma ; Fluorescence detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary A high performance liquid chromatographic method for the determination of flecainide in serum has been developed. The analysis is performed on a microparticulate silica column. The eluate is monitored by fluorescence detection at an excitation wavelength of 300nm and an emission wavelength of 370nm. No sources of interference were identified and a coefficient of variation of less than 8% was observed on repeated flecainide determinations. The method has a good reproducibility, specificity and accuracy, and can be applied in therapeutic drug monitoring of flecainide in patients.
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  • 59
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Coulometric electrochemical detection ; Methylnaltrexone ; Rat brain and serum analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple and sensitive method is described for the determination of methylaltrexone, a quaternary narcotic antagonist, in discrete rat brain regions and serum. Separation and quantitation are performed by reversedphase high-performance liquid chromatography with coulometric electrochemical detection. Perchloric acid extracts of the brain tissue or serum were passed through a normal-phase solid-phase extraction CN column, and methylnaltreexone was subsequently eluted with a mixture of absolute ethanol and 25mM trifluoroacetic acid. Methylnaltrexone gave a linear response over the range of 12.5–100ng in 1.0ml for cerebellar homogenates and 25–200ng in 50μl for serum. The average betweenassay coefficients of variation for methylnaltrexone from 1.0ml of cerebellar homogenate and 50μl of serum were 5.2 and 3.6%, respectively, over the concentration range studied. The within-assay coefficients of variation at 12.5ng/ml cerebellar homogenate and 25ng/50μl for serum were 7.4 and 4.6%, respectively. Analytical recovery of methylanyltrexone, added to cerebellar homogenate and serum samples, were 85 and 89%, respectively. The method was applied to the analysis of methylnaltrexone in discrete rat brain regions and serum after intraperitoneal injection.
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  • 60
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    Chromatographia 28 (1989), S. 129-132 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carotenoids ; Paprika, Rose hips, Marigold
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the preparative HPLC of carotenoids and carotenoid esters using a self-packing axially-compressed column. The reversed-phase system used employs an RP-18 stationary phase and a mobile phase consisting of a mixture of petroleum spirit, acetonitrile, methanol and tetrahydrofuran. The method is demonstrated for paprika fruit, rose hips and marigold flowers.
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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Wheat proteins ; γ-gliadins ; Effect of pH on separation ; Effect of organic modifier on separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Reversed-phase, high-pressure liquid chromatography has been used to separate similar protein (γ-gliadin) components from 70% ethanol extracts of endosperm flour from two different accessions of the diploid wheatTriticum monococcum L. The effect of acetonitrile as the organic eluent was compared to acetonitrile: 2-propanol (3:1) at two different pH's. Conditions for maximum resolution of the γ-gliadin components were found to be at pH 7.2 with acetonitrile: 2-propanol (3:1) as the eluent. These conditions allowed the components to be obtained in sufficient purity for further charaterization.
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  • 62
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand-exchange ; Preparative racemate resolution ; Amino-acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Preparative resolutions of racemic amino-acids by ligand-exchange chromatography are described. Base-line resolution of multigram quantities of many racemic solutes was obtained using very simple equipment (open tubular column).
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    Chromatographia 28 (1989), S. 354-358 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ternary mobile phases ; Solute retention model
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    Topics: Chemistry and Pharmacology
    Notes: Summary In our previous publications we have established a new physico-chemically grounded retention model valid for the adsorption and partition mechanism of retention using multicomponent mobile phases. Moreover, we have demonstrated its practical usefulness for predicting solute retention in several different chromatographic modes (i.e. in TLC, normal-phase and reversed-phase HPLC) employing binary mobile phases. In this paper we give an ultimate check to the physicochemical correctness of our new retention model, using it for the description of solute retention in reversedphase HPLC systems with ternary mobile phases of the B+AB1+AB2 type. The complexity of these mobile phases and of the possible intermolecular interactions among the consitituent solvents was supposed to rigidly scrutinize the premises of the assumed new approach. We have observed a good agreement between the experimental retention parameter for a number of solutes chromatographed with the use of two different mobile phases of the B+AB1+AB2 type, and the retention parameter calculated according to the assumed model. Therefore, we believe to have sufficiently tested our new approach and confirmed its physico-chemical correctness.
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Optical resolution ; Polymeric adsorbents ; Penicillin sulfoxide ; Substituent effect
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    Topics: Chemistry and Pharmacology
    Notes: Summary Fourteen new vinyl polymers carrying penicillin sulfoxide nucleus, poly (substituted-benzyl 1-oxo-6-metha-crylaminopenicillanate)s, were synthesized in order to investigate the influence of the substituents on the optical resolution capabilities. The resolution efficiency of the high-performance liquid chromatography columns comprising the obtained polymers were examined usingtrans-stilbene oxide and N-acetyl-1-phenethyl-amine. It was found that some columns resolved both racemates, some one, while the others did not separate either. A polymer which has 2,6-dichlorobenzyl moiety was found to resolve both racemates more effectively than the unsubstituted polymer.
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  • 65
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    Chromatographia 28 (1989), S. 465-468 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chlorinated phenols ; 4-Aminoantipyrine derivatives of phenols ; Metabolites of phenoxy alkanoic acid herbicides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High performance liquid chromatography (HPLC) has been applied to the separation and determination of o-chlorophenol, 2,4-dichlorophenol, 3,4-dichlorophenol, 2,5-dichlorophenol, and 2,4,5-trichlorophenol in water samples after prior derivatization with 4-aminoantipyrine. These substances are the phenolic decomposition products of the phenoxy-alkanoic acid herbicides: 2,4-dichlorophenoxyacetic acid (2,4-D), 2,4-dichlorophenoxybutyric acid (2,4-DB), and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T). An RP-C18 column was used, with gradient elution starting at 50/50 and changing to 70/30 methanol/water (v/v) after 24 min. Detection was carried out at 470 nm where the 4-aminoantipyrilquinonimine derivatives show maximum absorbance. The method was linear over a concentration range of 5–10,000 ppb phenol in the original water sample. By using an enrichment step a detection limit of 2 ppb phenol could be approached. The method was used to study the degree of degradation of the phenoxy acids to phenols under different conditions of temperature, pH, and UV irradiation.
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  • 66
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand exchange ; Chiral phase ; Optical resolution of 2-hydroxy acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Using an MCl GEL CRS10W column, which was packed with octadecyl silica (ODS) coated with N,N-dioctyl-L-alanine, optical resolution of 2-hydroxy acids was performed. The optical resolution of mandelic acid derivatives and C2 to C5 2-hydroxy acids was carried without any pretreatment. The MCl GEL CRS10W column could resolve amino acids and 2-hydroxy acids. For their selective detection, a post-column method was employed in which the specific color reaction of 2-hydroxy acids with iron(III) ion was utilized. For the analysis of foodstuffs, in which amino acids and 2-hydroxy acids often coexist, the present method was found to be effective in distinguishing between these enantiomers.
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  • 67
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    Chromatographia 28 (1989), S. 497-501 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Collagen metabolites ; Amino acid derivatives ; Glycosides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Methods are described for the isolation of galactosyl hydroxylysine and glucosylgalactosyl hydroxylysine from collagen and for the quantitative analysis of these hydroxylysine glycosides. The isolation procedure, based upon gel filtration and preparative ionpaired reversed-phase high-performance liquid chromatography, is simple and rapid in comparison with existing methods, allowing the production of tens of milligrams of each glycoside in a single day. Quantitative analysis of the hydroxylysine glycosides is effected by reversed-phase high-performance liquid chromatography with precolumn derivatization (usingo-phthal-dialdehyde) and fluorescence detection.
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  • 68
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Optical resolution ; Polymeric adsorbents ; Penicillin sulfoxide ; Copolymerization
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    Topics: Chemistry and Pharmacology
    Notes: Summary A methacrylamide carrying penicillin sulfoxide skeleton, benzyl 1-oxo-6-methacrylaminopenicillanate, was copolymerized with methyl methacrylate. The optical resolution efficiency of the columns comprising the obtained copolymers was investigated using a high-performance liquid chromatography system. A copolymer incorporated by 27mol% of methyl methacrylate showed higher chirality recognition capability than the homopolymer, which suggests that the introduction of methyl methacrylate contributes to enriching desired penicillin sulfoxide alignment (i. e., tracticity) along the polymer main chain. An estimated penicillin monomer's number-average sequence length in the copolymer was 2.7.
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  • 69
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    Chromatographia 28 (1989), S. 519-522 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase chromatography ; Separation of metal acetylacetonates
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    Topics: Chemistry and Pharmacology
    Notes: Summary Using reversed-phase high-performance liquid chromatography acetylacetonate complexes with trivalent metals such as Al(III), Co(III), Cr(III) and Fe(III) have been examined in columns containing RP-2, RP-8 and RP-18 bonded phases. The mobile phase consisted of acetonitrile/water or methanol/water mixtures with various compositions. As shown the order of elution of the acetylacetonates depends on the type of the column packing and on the nature and concentration of the organic modifier in the mobile phase.
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  • 70
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Penstemide and serrulatoloside
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    Topics: Chemistry and Pharmacology
    Notes: Summary Penstemide and serrulatoloside, two iridoids of similar molecular structure, were separated by stepwise gradient TLC in a straight-phase systems (silica-ethyl acetate+isopropanol) and by HPLC in a reversed-phase system (ODS-silica — water+methanol).
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  • 71
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Overpressured layer chromatography ; Furocoumarin isomers ; Preparative separation of plant extracts
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    Topics: Chemistry and Pharmacology
    Notes: Summary Preparative medium pressure liquid chromatography and semi-preparative high performance liquid chromatography on silica were employed for the isolation of eight furocoumarin isomers (iso-bergapten, angelicin, psoralen, bergapten, pimpinellin, sphondin, xanthotoxin and isopimpinellin). The conditions were transposed from analytical on-line overpressured layer chromatography and analytical high performance liquid chromatography, respectively. The retention data of the analytical on-line overpressured layer chromatographic separation and the preparative medium pressure liquid chromatographic isolation show a linear relationship. Using 15 μm TLC silica 60 as stationary phase a dry-packing procedure aas developed for labomatic medium pressure liquid chromatographic glass columns. The efficiency of the preparative separation techniques was demonstrated by the isolation of the investigated furocoumarins from Heraclei mantegazziani radix and from Pimpinellae radix (Balkan quality).
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  • 72
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    Chromatographia 27 (1989), S. 101-104 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bromo/iodosubstituted thyronines ; Mobile phase optimization ; Radioimmunoassay detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase high performance liquid chromatographic method on C-18 bonded silica is described for the separation of trisubstituted iodo/bromothyronines, which exert thyroid hormone activity. The composition of the mobile phase has been systematically optimized resulting in a ternary mixture of methanol/acetonitrile/water acidified with trifluoroacetic acid. The applicability of ultraviolet absorption detection, amperometric detection and off-line radioimmunoassay was investigated. The latter method allows detection of the different iodo/bromothyronines down to 40–120 ng/l mobile phase; this sensitivity is high enough for application to thyroid hydrolysates in order to clarify the question as to whether bromine can substitute iodine in the biosynthesis of thyroid hormones.
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  • 73
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    Chromatographia 27 (1989), S. 113-117 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention contribution of nitrogen ; Effect on methylene and sulphur chains
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    Topics: Chemistry and Pharmacology
    Notes: Summary The reaction of secondary amines R2NH with disulfur dichloride S2Cl2 in dichloro methane yields mixtures of bis-dialkylamino polysulphides R2N−Sn−NR2 with sulphur chain lengths varying from ns=2 to 14. The S chains are believed to be non-branched. The compounds form homologous series in each of which sulphur atoms give a constant contribution to retention. The sulphur retention index depends slightly on the carbon number in the terminal alkyl groups R. The presence of nitrogen lowers retention. The index increment of N is ca. −160 units, which is distinctly less negative than values found in alkylamines.
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  • 74
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size-exclusion chromatography ; Fast atom bombardment-MS ; Peptic haemoglobin hydrolysate
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the ready identification of any peptide isolated from a complex peptic haemoglobin hydrolysate produced on the pilot-plant scale. A combination of size exclusion and reversed-phase, high-performance liquid chromatography have proved to be a useful strategy for fractionation of such a mixture. This technique enabled pure peptides from the total hydrolysate to be obtained. Amino acid analysis and fast atom bombardment mass spectrometry provided the accurate composition and molecular weight of any isolated peptide. Molecular weights are compared with those deduced from size-exclusion chromatography (SEC) and the usefulness of SEC is discussed. The procedure described in this study will be useful for acquiring a better knowledge of such an hydrolysate and could be extended to other crude protein digests.
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  • 75
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrochemical detector ; Amines ; Silages ; Feedstuffs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of the electrochemical detector (EC) in the high performance liquid chromatography (HPLC) of dansyl derivatives of biogenic amines is reported. Isocratic and gradient elution patterns of synthetic mixtures of putrescine, cadaverine, 1,6-diaminohexane, tryptamine, histamine, tyramine, spermine and spermidine on a reversed phase column are shown. Hydrodynamic voltammograms of standard compounds are presented. The detection limits of the EC are compared with those of ultraviolet and spectrofluorimetric detectors. A chromatographic profile of amines from the proteolytic catabolism of maize silage byClostridia is shown.
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  • 76
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase elution ; Silica and cyano columns ; Flavonoid compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary HPLC retention data for a number of flavonoid compounds have been evaluated on normal phase silica and cyano colums according to the Soczewinski-Snyder (S.-S.) model. On the silica phase most of the flavones examined exhibited asymetrical peak shapes indicating strong and mixed retention mechanisms; on the cyano phase the intercept of the S.-S. relationship was independent of any hydroxy substitution pattern or of molecular planarity. A similar behaviour, but with different intercept values, was observed with coumarin and quinone compounds.
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  • 77
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    Chromatographia 27 (1989), S. 292-296 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Selenium(IV)-tellurium(IV) separation ; Flow-through coulometric detector
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    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic behaviour of selenium and tellurium has been investigated with two different reversed-phase chromatographic methods, using P-350 (methyl-bi-isooctyl phosphate) and TBP (tributyl phosphate) as the stationary phases. HCl, HBr, NaCl and NaBr were employed as mobile phase components in both methods. The results suggested that the separation mechanism corresponds to the formation of TeCl (or TeBr) and P-350H (or TBPH) ion associate. A coulometric flow-through detector was applied to determine Se(IV) and Te(IV). Complete separation and quantitative determination of Se and Te could be achieved in 10 minutes.
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  • 78
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    Chromatographia 27 (1989), S. 325-327 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carotenoid ; Xanthophyll ; Broccoli ; Paprika
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the preparative HPLC of up to 50mg of carotenoid using a self-packing axially-compressed column. Oxygenated carotenoids, xanthophylls, are separated with silica as the stationary phase and acetone/petroleum ether as the mobile phase, while carotenes are separated using magnesium oxide/polyamide as the stationary phase and undiluted petroleum ether as the mobile phase.
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  • 79
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    Chromatographia 27 (1989), S. 340-342 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Evaporative light scattering detection ; α, ω-Dicarboxylic and hydroxycarboxylic acids ; Alkylglucosides and glycerides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The advantages of an evaporative light scattering detector in HPLC are demonstrated using the separation of α, ω-dicarboxylic and hydroxycarboxylic acids, alkyl glucosides and mono-, di- and triglycerides as examples. By using this detector reversed phase as well as normal phase gradient HPLC becomes possible for substances with no UV absorption.
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  • 80
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    Chromatographia 27 (1989), S. 371-377 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Alkyl-bonded silica gel ; Enthalpy ; Van der Waals volume
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    Topics: Chemistry and Pharmacology
    Notes: Summary Starting from silica gel with a purity of 99.999%, octadecyl-(ODS), octyl-(C8) and propyl-(C3) bonded silica gels were synthesized, and end-capped by trimethyl groups. The pore size was 150 Å and the specific surface area was 320 m2/g. The ODS and C8 silica gels were stable in both acidic and basic solutions. The selectivity of these bonded-silica gels was examined from the difference of the retention behavior of alkanes (Al−Al), alkylbenzenes (Ph−Al), alkylalcohols (Al−OH) and polyaromatic hydrocarbons (PAH) in aqueous acetonitrile. On these packings the log k′ values decreased in the order Al−Al〉Ph−Al〉PAH〉Al−OH. Furthermore, the chromatographic behavior of these compounds was measured on polymer-coated octadecyl-bonded silica gel (CAP) and octadecyl-bonded vinyl alcohol copolymer gel (ODP). The selectivity was verified from the value of R* of these compounds: $$R = R_v + R^* $$ where R is the retention time, and Rv is the retention time of an alkane having the same Van der Waals volume as the analyte. The R* values indicated that this ODS had more selectivity than C8 and C3, however R* on C8 showed a very good correlation with R* on C3. Their retention behavior on CAP was similar to that of ODS, however, their capacity ratios measured on CAP were smaller than those on ODS. The ODP has selectivity for the retention of aromatic compounds, because PAHs were retained strongly on this column.
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  • 81
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Alternaria mycotoxins ; Food analysis ; Electrochemical detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The electroactivity of majorAlternaria mycotoxins has been explored in order to devise a liquid chromatographic-electrochemical detection (LC-EC) method for the determination of these toxic metabolites in fungal cultures and in naturally contaminated foodstuffs. Alternariol, alternariol methyl ether, altertoxin-I and altertoxin-II have been found to be electroactive and could be detected at sub-nanogram levels. Advantages and limitations of dual electrode (screen mode) coulometric detection and single electrode amperometric detection are presented and discussed. The feasibility of electrochemical detection in gradient elution liquid chromatography as well as its applicability to the analysis of contaminated foodstuffs is demonstrated.
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  • 82
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    Chromatographia 27 (1989), S. 431-435 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; UV diode array detection ; Electro chemical detection ; Herbicides
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    Topics: Chemistry and Pharmacology
    Notes: Summary An automated procedure is described for simultaneous UV detection at three different wavelengths and electro chemical detection in series of some residual herbicides. UV spectra of nine compounds of different compound groups are presented. Liquid-liquid extraction with dichloromethane and an enrichment of about one thousandfold has been used. Recovery rates after enrichment and detection limits of four s-triazine, three phenyl urea herbicides, metazachlore and metamitrone in river and drinking water are shown. It is concluded that the herbicides examined can be detected at levels between 10ng l−1 and 50ngl−1, without the necessity of derivatisation or clean-up processes.
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  • 83
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    Chromatographia 27 (1989), S. 257-263 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size exclusion ; Fractal dimension ; Retention model
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    Topics: Chemistry and Pharmacology
    Notes: Summary Some porous packings used in chromatography have been claimed to be fractals with a scale of sizes a〈l〈L, where a is a molecular size and L is the size of the largest pores. For a fractal porous packing, the excluded volume for molecules in solution in the vicinity of the packing surface is directly related to Df, the fractal dimension of the pore surface (2〈Df〈3). Since retention in size exclusion chromatography is itself directly related to this excluded volume, the fractal nature of the packing provides a model of retention in this technique. According to this model there is a linear relationship between log Rs and log(1-Kd), where Rs is the hydrodynamic radius of the solute macromolecules and Kd the distribution coefficient. The fractal dimension is derived from the slope of this plot. Size exclusion chromatographic retention data have been analyzed according to the model. It is found that some HPLC packings are fractals with fractal dimensions ranging from about 2.15 to 2.6, depending on the material. Such a large range of Df values indicates large variations in the selectivities and domains of applications of the different packings. For some classical gel filtration chromatographic gels, the fractal retention model does not seem to apply.
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  • 84
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micro-columns ; Flow rate and temperature programming ; PTH amino acid derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of phenylthiohydantoin (PTH) amino acid derivatives by flow rate and temperature programming in reversed-phase micro-column liquid chromatography (LC) has been investigated. For both programming modes a microcomputer-assisted retention prediction system (REPRES) was constructed. The performance of this system has been evaluated by comparing actually measured retention data to those predicted. Excellent agreements between those data were found. It is clearly indicated that simultaneous flow rate and temperature programming can improve the separation of PTH-amino acids in reduced analysis time.
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  • 85
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    Chromatographia 28 (1989), S. 89-91 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrophoresis ; Comparison of HPLC and electrophoresis ; Proteins, peptides and amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Protein structure analysis is an indispensible tool in modern biological research. However, the isolation of a protein or the separation of peptides in a form suitable for sequence analysis is a considerable technical challenge. The two predominant separation methods in protein biochemistry are chromatography and electrophoresis. In this paper the position, advantaged and disadvantages of both HPLC and electrophoresis for the separation of amino acids, peptides and proteins in protein structure analysis are discussed.
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  • 86
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    Chromatographia 28 (1989), S. 565-568 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; New bonded phases ; Alumina ; Protein separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Several reactions are tested for the chemical modification of alumina. These include the following: chlorination of the surface hydroxyls followed by reaction with an organolithium compound; chlorination of the surface hydroxyls followed by reaction with a Grignard reagent; chlorination of the surface hydroxyls followed by reaction with an amine; chlorination of the surface hydroxyls followed by reaction with an alcohol; direct reaction of the alumina with an organochloroalane and direct reaction of the alumina with an alcohol. Only the first reaction gave a product which contained enough bonded organic material to be easily detected by FTIR. Preliminary stability tests show that the product of the first reaction retains the bonded organic material when exposed to nonpolar and polar organic solvents as well as aqueous solutions of pH 1.0, 7.0 and 12.0. Chromatographic testing establishes reversed-phase behavior for alkylarylketones as solutes and the bonded phase displays good biocompatibility for a series of protein standards.
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  • 87
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adenosine phosphates ; Adenosine phosphate degradation products ; Innervated frog muscle
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Adenosine mono-, di- and triphosphates, inosine monophosphates, adenosine, inosine and hypoxanthine were separated in a single run by high-performance liquid chromatography with UV detection. AC-18 reversephase column was used. An isocratic elution with 100mM phosphate buffer (KH2PO4) pH6.5 and 1.2% methanol, followed by a 5 minute linear gradient up to 15% methanol after the 10th minute was performed during each run with a flow rate of 1.25ml/min. The time required for each analysis was 25 minutes. The detection limit for each substance ranged from 3 to 5 pmol. All the substances under study were detected in the incubation medium when adenosine triphosphate was exogenously applied to the innervated frog sartorius muscle.
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  • 88
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Molecular interactions ; Association effects ; Analyte solvation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The linear Jaroniec equation has been utilized for the description of chromatographic systems in which the test substance molecule is solvated by the solvent molecules. A possibility of the formation of multimolecular solvates in the bulk phase has been confirmed. The measurements were made using liquid adsorption chromatography with ternary mobile phase.
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  • 89
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral separations ; Trypsin on silica ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new HPLC stationary phase was synthesized by the covalent immobilization of the enzyme trypsin (TRYP) on silica. The hydrolytic activity of the immobilized enzyme was 72% of the activity of an equivalent molar amount of free TRYP. The initial chromatographic studies indicate that this phase can be used for chiral separations of enantiomeric O- and N,O-derivatized amino acids which are natural substrates on TRYP and that the stereochemical resolutions are a result of the activity of the enzyme.
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  • 90
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    Chromatographia 28 (1989), S. 574-578 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases ; End-capping ; Destructive effects on bonded phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMS) have been used as a secondary deactivation (end-capping) reagents for packing materials for RP HPLC. Three types of chemically bonded phases (CBP) with different structures and different coverage densities were used. The destructive effects of HMDS on the coverage density of chemically bonded C18 and C8 phases is discussed.
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  • 91
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cellulose acetate ; Acetyl content ; Temperature effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Cellulose and cellulose mono-, di-, and triacetate were used as stationary phases for liquid chromatography with water as a mobile phase, and the retention behavior of alcohols, ethers, ketones, and chlorides was examined. For cellulose acetate columns, the logarithm of the specific retention volume, (logV g * ), correlated linearly with the logarithm of partition coefficient between 1-octanol and water (log Ko/w), for each homologous group, but all solutes were unretained on cellulose columns. With the exception of chlorides, the intercept values of the log V g * –log Ko/w regression lines increased significantly with increase of acetyl content of cellulose acetates, but the slopes of the regression lines changed little. This suggests that hydrophobic interaction between the acetyl groups of cellulose acetates and the alkyl chains of the solutes is the dominant factor in the retention. The capacity factors for 1-alcohols with cellulos diacetate column indicated a maximum at a column temperature of about 40°C. This unique retention behavior was assumed to be caused by small structural change of the cellulose acetate polymer, because this temperature effect on the retention corresponded with effects observed by differential scanning calorimetry (DSC).
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  • 92
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    Chromatographia 28 (1989), S. 161-166 
    ISSN: 1612-1112
    Keywords: Thin-layer chromatography ; Column liquid chromatography ; Micropreparative separations ; Furocoumarins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Furocoumarins from extracts ofHeracleum genus fruits were separated using normal and reversed phase TLC and HPLC and isolated in the milligram scale using overloaded systems of column chromatography. Binary or ternary solvents containing a polar modifier (methanol, diisopropyl ether or acetonitrile) were used as the mobile phases.
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  • 93
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange ; Mobile phase optimisation ; Egg-white proteins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Factors influencing the capacity of Whatman QA52 anion-exchange cellulose for hen egg-white proteins have been investigated. While simply increasing the concentration of protein in the feedstock increases the loading there is a concomitant reduction in binding efficiency in a single pass through the column. Substitution of buffer by water in the mobile phase during sample preparation, thereby reducing the ionic strength of the feedstock, had the effect of significantly increasing protein capacity whilst improving binding efficiency. During column loading large changes in pH of the mobile phase were observed although this had no apparent effect on the chromatography for this system.
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  • 94
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    Chromatographia 28 (1989), S. 193-196 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phases ; Immobilized enzymes ; Racemic resolution of amino acid esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Racemic resolution of aromatic and aliphatic amino acid esters into L-amino acid and D-amino acid ester via LC and HPLC is achieved by using enzyme reactors as chromatographic columns. For this purpose α-chymotrypsin and trypsin are immobilized on Eupergit C, Sepharose 4B and Lichrosorb-Diol.
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  • 95
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bonded stationary phases ; Evaluation of the hydrophobicity of sorbents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The energy of interaction (∈0) between the methylene group and the surface of a sorbent is proposed for use in the quantitative evaluation of the hydrophobicity of a sorbent. A method was developed to determine the ∈0 parameter from chromatographic measurements using the investigated sorbent as the stationary phase and linear methylene-containing homologous series, e.g., alkanols, amino-alkanes, etc., as the test compounds. The effectiveness of this method is demonstrated by using, as examples, a series of bonded stationary phases and a series of cross-linked copolymeric sorbents differing in the concentration of the hydrophobic groups. The proposed method is compared with the Martin rule used extensively in the chromatography of oligomers.
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  • 96
    ISSN: 1612-1112
    Keywords: Thin-layer chromatography ; Column liquid chromatography ; Mobile phase optimization ; HPTLC transposition to HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A computer-assisted method is presented for mobile phase selection for the optimal separation of pesticides by HPTLC and HPLC. The system is based on a plot of solute retention value and separation criterion vs. binary mobile phase composition for graphic optimization. The result of HPTLC can be transposed to HPLC for optimal separation. The transposition equation is given.
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  • 97
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    Chromatographia 28 (1989), S. 311-312 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flavonoid glycosides ; Betula
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The main flavonoid glycosides ofBetulae folium extracts (quercetin-3-glucuronide, myricetin-3-galactoside, hyperosid, quercetin-3-arabinoside and quercetin-3-rhamnoside) have been separated by isocratic elution on a C18 Aquapore RP-300 column. Elution was performed with 17% isopropanol at pH 6.2 confirming the validity of this eluent for the analysis of the flavonoid glycosides.
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  • 98
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phase ; Resolution of amino acid derivatives ; Enantioseparation by HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chiral stationary phase for the separation of some D-and L-amino acid derivatives using a new resolving agent is described. The enantiomeric resolution was accomplished by normal phase high-performance liquid chromatography. The support was easily prepared by coating an epoxy polymer of L-valinamide on aminopropylsilanized macroporous silica. The influence of subambient temperatures on the enantioselectivity was also examined.
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  • 99
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral recognition process ; Enantiomeric elution order ; Mobile phase modifiers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Three enantiomeric solutes, a sulphoxide, a piperidine derivative and a methyl ester have been chromatographed on an HPLC chiral stationary phase (CSP) based upon cellulose-tribenzoate (Chiralcel OB-CSP). The mobile phases used in the study were composed of hexane modified with homologous series of primary, secondary and cyclic alcohols. Interesting reversals in enantiomeric elution order have been observed for 2-phenoxypropanoic acid methyl ester associated with changes in chain length or ring size of the alcohol mobile phase modifier. The results of the study suggest that at least two chiral recognition mechanisms operate on the OB-CSP and point out the importance of acquiring elution order data in all studies involving chiral stationary phases.
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  • 100
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Prediction of retention times ; Gradient elution ; Substituted quinolines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chromatographic model able to predict, from experimental isocratic data, retention times of solutes under gradient conditions has been proposed previously. The prediction was shown to be totally independent of the chemical properties of both solutes and eluents. In order to further check the general validity of the theory, the model has now been applied to a nonhomologous set of compounds, namely a range of substituted quinolines (methyl-, hydroxy- and amino-) and several different stationary phases. Results show a dependence on the stationary phase and, to a lesser extent, on the chemical structure of the solutes. The possible sources of errors are discussed. The generality of the method holds, within acceptable limits, if predictions concern the same type of stationary phase.
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